US3099537A - Process for the treatment of an organic solvent containing uranium - Google Patents

Process for the treatment of an organic solvent containing uranium Download PDF

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Publication number
US3099537A
US3099537A US77009658A US3099537A US 3099537 A US3099537 A US 3099537A US 77009658 A US77009658 A US 77009658A US 3099537 A US3099537 A US 3099537A
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United States
Prior art keywords
uranium
solvent
column
organic solvent
solution
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English (en)
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Mason Harold
Sanderson James Roland
Mason Tony
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UK Atomic Energy Authority
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UK Atomic Energy Authority
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    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21C—NUCLEAR REACTORS
    • G21C19/00—Arrangements for treating, for handling, or for facilitating the handling of, fuel or other materials which are used within the reactor, e.g. within its pressure vessel
    • G21C19/42—Reprocessing of irradiated fuel
    • G21C19/44—Reprocessing of irradiated fuel of irradiated solid fuel
    • G21C19/46—Aqueous processes, e.g. by using organic extraction means, including the regeneration of these means
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/30—Nuclear fission reactors
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies

Definitions

  • uranium content of all efiluent from a production plant using uranium should be accurately measured at frequent intervals and that the results should be presented to the plant operator within a few minutes of the sample being taken so that plant operation can be corrected, if necessary, before loss of uranium reaches substantial proportions.
  • a process for the treatment of an organic solvent containing uranium comprises the steps of washing the solvent with an aqueous solution of a colorimetric agent for uranium so as to bring substantially all the uranium into the aqueous solution, treating at least part of the colored aqueous solution with a decolorizing agent for the coloration due to uranium only and measuring the difference between color intensity before and after treatment with the decolorizing agent.
  • any uranium in the aqueous solution is transferred to an organic solvent by a conventional solvent extraction step and the test of the invention is then carried out on the organic phase. If necessary a salting agent is added to the original aqueous solution to ensure that substantially all the uranium is transferred to the organic phase.
  • the preferred organic solvent is tributyl phosphate diluted with odorless kerosene and the preferred salting agent nitric acid,
  • a preferred colorimetric agent is ammonium thioglycollate solution which converts any uranium in the organic solvent to uranium thioglycollate having an intense yellow color.
  • This uranium thioglycollate may be destroyed by carbonate ions yielding a colorless double carbonate of uranium and ammonia.
  • the carbonate ion may be added as carbon dioxide or ammonium carbonate but carbon dioxide is preferred as the decoloration step does not then lead to any volume change in the thioglycollate solution and comparative measurement of the color intensity is therefore easier.
  • a suitable method of complexing thorium is to wash the organic solvent with a neutral solution of a complexing agent such as the sodium salt of ethylene diamine tetra acetic acid.
  • FIG. 1 shows the injection and extraction system
  • FIG. 2 shows the mechanism for controlling the rate of liquid flow to the system of FIG. 1;
  • FIG. 3 shows the absorptiornetric cell unit.
  • the apparatus of FIG. 1 comprises essentially a forward extraction column 10 and a backward extraction column 11.
  • the column 10 is fed with aqueous sample from the dispenser 1-2 and with organic solvent from the dispenser 13 (via the pipes 28, 29, respectively).
  • the column 11 is fed with organic solvent phase from column 10 via the pipe 14 and with ammonium thioglycollate solution from the dispenser 15 via the pipe 30.
  • the dispensers 12, 13, 15 are more fully described in copending US application Serial No. 770,097.
  • a constant head is maintained in the sample dispenser 12 by an overflow pipe 16 and in the dispensers 13 and 15 by float chambers 17 and 18, respectively.
  • the columns are of the rotary type described in United States Patent No.
  • aqueous phase leaves the column 10 via a siphon arm 20 which dips into a small secondary vessel 21 constituting the controller for the static interface, that is, the position of the interface in the column 10 when the feed solutions are flowing but the rotor is stopped, and having an outlet 22 from which the aqueous phase drips to waste.
  • aqueous phase flows via a siphon arm 23 -to a subsidiary settling vessel 24 which constitutes a static interface controller for the column 11 and has an outlet 25 to waste for any organic phase carried into the vessel 24 and an outlet 26 to an absonptiometer (FIG. 3) for the uranium containing aqueous phase.
  • the solvent phase leaves the column 11 by a pipe 27 and can be recovered for re-use if desired.
  • each vortex consisting of a series of small globules of solvent which slowly rise through the continuous aqueous phase until they reach the annular setting space around the bearing 19b.
  • a mixture of solvent and aqueous phase is carried some distance up the annular space before final separation occurs and this point is shown as a well-defined interface line termed the dynamic interface.
  • This position of this interface is determined by the flow-rates used, the rotor speed and the positions of the static interface.
  • the dynamic interface is just above the aqueous inlet port and small adjustments can be made with the static interface controller to set it at the correct level.
  • the column 11 is adjusted similarly to the column 10 except that in the column 11 the solvent phase is continuous and the static interface is set at a point about one inch above the top of the bearing 19c. On starting the rotor the dynamic interface should be obtained as a layer of solvent A" below the bearing 19c.
  • the position of the interfaces in each column will also depend on the flow rates of the feed solutions. Using a sample feed 3 to 5 normal with respect to nitric acid an organic solvent feed of v./v. tributyl phosphate in odorless kerosene and a backwash feed of 0.4% v./v. solution of thioglycollic acid in 5% v./v. ammonium hydroxide flow rates of 6 ml./min.
  • the feed rates of the solutions fed to columns 10 and 11 is controlled by the cam mechanism shown in FIG. 2, which operates plungers 41 in the dispensers 12, 13 and 15.
  • Cams 42 are mounted on a cam shaft 43 running between bearings 44 and driven by a motor 45.
  • the cams 42 depress the plungers 41 about 80 times a minute to allow liquid to flow into the feed pipes for the columns 10 and 11.
  • the rate of feed will depend on the frequency at which the plungers 41 are depressed, and the extent and time they are depressed on each cycle.
  • the frequency and time of depression is governed by the speed of rotation of the shaft 43 and the shape of the cams 42 and the extent that the plungers are depressed is adjusted by means of wedges 50 so that the feed rates for the different solutions may be varied individually.
  • the size of the capillary delivery tubes from the dispensers is as large as possible subject to the requirement that they even out the liquid flow past the plungers 41.
  • the motor 45 is energized from supply terminals 51 via a manually controlled switch 46 and a switch 48 operated by a cam 47 on the cam shaft 43.
  • the switches 46 and 48 are in parallel.
  • the cam switch 48 is arranged to be closed (i.e. the motor energized) so long as any of the plungers 41 are depressed so that the motor cannot be stopped in a position which will allow flow of liquid past a depressed plunger.
  • the absorptiometer shown in FIG. 3 comprises two 1 cm. cells 31, 32 fitted respectively with inlet tubes 33, 34
  • vent tubes 39 are provided. In the event of line blockage liquid builds up in the vent tubes 39 and can only overflow at a point outside the absorptiometer.
  • the aqueous solution from the column 11 should pass first through one cell of the absorptiometer and then through the other. It is possible to divert the flow of colored solution so that part flows through one cell and part is decolorized before flowing through the other cell but in that case the relative volumes of the two parts must be carefully controlled. It is also possible to arrange for the solution from more than one extraction system to be fed into the same absorptiometer, solution being allowed to flow into the absorptiometer cells from each extraction system in turn.
  • a process for measuring the uranium content of an organic solvent having uranium and other impurities present therein comprising washing the solvent with a solution of a salt of thioglycollic acid to produce a colored complex of uranium thioglycol'late and other impurities in said solvent, treating at least a portion of said treated solvent with a material capable of imparting carbonate ions therein to convert only the uranium thioglycollate complex into a colorless state, measuring the difference between color intensity before and after treatment with said carbonate ion imparting agent by said color differentiation, and determining the amount of uranium present in said solvent by said color differentiation.
  • a process in accordance with claim 1, wherein the material capable of imparting carbonate ions is carbon dioxide.
  • a process for measuring the uranium content of an organic solvent having uranium and other impurities present therein comprising Washing the solvent with a solution of a salt of .thioglycollic acid to produce a colored complex of uranium thioglycollate and other impurities in said solvent, measuring the color intensity of said solvent, treating said treated solvent with a material capable of imparting carbonate ions therein to convert only the uranium thioglycol'late complex into a colorless state, measuring the color intensity of said solvent, determining the difference between the color intensity of the first stage and the second stage, and determining the amount of uranium present in said solvent by said color differentiation.
  • a process for measuring the uranium content of an aqueous uranium bearing solution having other interruptionities therein comprising treating the aqueous solution with tributyl phosphate to extract the uranium and other impurities in the tributyl phosphate phase, washing the tributyl phosphate phase containing uranium with ammonium thioglycollate to produce a colored complex or uranium thioglycoll ate and other impurities in said tributyl phosphate phase, treating at least a portion of said tributyl phosphate phase With carbon dioxide to convert only the uranium thioglycollate complex into a colorless phase, measuring the difference between the color intensity before and after the treatment with said carbon dioxide by said color differentiation, and determining the amount of uranium present in said solvent by said color differentiation.

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Plasma & Fusion (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Extraction Or Liquid Replacement (AREA)
US77009658 1957-10-31 1958-10-28 Process for the treatment of an organic solvent containing uranium Expired - Lifetime US3099537A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB3408057A GB868137A (en) 1957-10-31 1957-10-31 Improvements in or relating to a method of testing for uranium and apparatus therefor

Publications (1)

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US3099537A true US3099537A (en) 1963-07-30

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US77009658 Expired - Lifetime US3099537A (en) 1957-10-31 1958-10-28 Process for the treatment of an organic solvent containing uranium

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US (1) US3099537A (de)
BE (1) BE572490A (de)
DE (1) DE1208521B (de)
FR (1) FR1212522A (de)
GB (1) GB868137A (de)
NL (1) NL113020C (de)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3403004A (en) * 1963-11-29 1968-09-24 Yissum Res Dev Co Means and method for the detection of uranium
US4349350A (en) * 1980-03-17 1982-09-14 Commissariat A L'energie Atomique Process for the determination of uranium (VI) or dialkyl dithiophosphoric acid present in an organic solvent
US5424211A (en) * 1994-05-16 1995-06-13 The United States Of America As Represented By The United States Department Of Energy Composition for detecting uranyl
CN103395759A (zh) * 2013-08-02 2013-11-20 柳州化工股份有限公司 一种配制硝酸水溶液脱色方法
CN103395758A (zh) * 2013-08-02 2013-11-20 柳州化工股份有限公司 一种配制硝酸水溶液的装置

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2019871A (en) * 1933-08-26 1935-11-05 Pettingill Clark Continuous oxygen recorder

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2474007A (en) * 1945-06-21 1949-06-21 Shell Dev Method of and apparatus for contacting fluids
GB793806A (en) * 1955-07-05 1958-04-23 Atomic Energy Authority Uk Improvements in or relating to optical absorptiometers

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2019871A (en) * 1933-08-26 1935-11-05 Pettingill Clark Continuous oxygen recorder

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3403004A (en) * 1963-11-29 1968-09-24 Yissum Res Dev Co Means and method for the detection of uranium
US4349350A (en) * 1980-03-17 1982-09-14 Commissariat A L'energie Atomique Process for the determination of uranium (VI) or dialkyl dithiophosphoric acid present in an organic solvent
US5424211A (en) * 1994-05-16 1995-06-13 The United States Of America As Represented By The United States Department Of Energy Composition for detecting uranyl
CN103395759A (zh) * 2013-08-02 2013-11-20 柳州化工股份有限公司 一种配制硝酸水溶液脱色方法
CN103395758A (zh) * 2013-08-02 2013-11-20 柳州化工股份有限公司 一种配制硝酸水溶液的装置
CN103395759B (zh) * 2013-08-02 2015-01-14 柳州化工股份有限公司 一种配制硝酸水溶液脱色方法

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Publication number Publication date
GB868137A (en) 1961-05-17
BE572490A (de) 1900-01-01
NL113020C (de) 1900-01-01
DE1208521B (de) 1966-01-05
FR1212522A (fr) 1960-03-24

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